Reaktion #1148621

ord-33f6df645d154677aa5c5b80a33a661c

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONthe reaction solution was distilled off under reduced pressure
  2. 2
    workup.DISSOLUTIONThe resulting residue was dissolved in chloroform
  3. 3
    Waschenwashed with saturated sodium bicarbonate solution, and saturated salt water
  4. 4
    Trocknendried over anhydrous sodium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Vorschrift

36.98 g of 4-chloro-3-methoxy-2-methylpyridine (V) was dissolved in 685 ml of acetic acid and 92 ml of hydrogen peroxide water was added thereto and the resulting mixture was heated at 90° C. for 24 hours, and thereafter, the reaction solution was distilled off under reduced pressure. The resulting residue was dissolved in chloroform and washed with saturated sodium bicarbonate solution, and saturated salt water, and thereafter, dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 37.64 g of 4-chloro-3-methoxy-2-methylpyridine N-oxide (VI).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06525066B2uspto-grants-2003_02